Sodium Hydroxide → 2-Azido-2-methoxyacetic acid

HRID 1658004ノート

反応式

HRID 1658004 の反応式
[OH-].[Na+].[N:3]([CH:6]([O:11][CH3:12])[C:7]([O:9]C)=[O:8])=[N+:4]=[N-:5]>CO>[N:3]([CH:6]([O:11][CH3:12])[C:7]([OH:9])=[O:8])=[N+:4]=[N-:5]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 20357785Methyl 2-azido-2-methoxyacetate

生成物 1

HCID 215299592-Azido-2-methoxyacetic acid収率 93.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Aqueous sodium hydroxide (30 ml. of a 2.5 N solution) is added dropwise over 15 minutes to a stirring solution of methyl 2-azido-2-methoxyacetate (10.40 g., 72 mmole) in methanol (8.5 ml.). The mixture becomes warm and cloudy during the addition. The methanol is removed under reduced pressure and the aqueous residue is acidified to pH 1 with concentrated sulfuric acid and extracted with ether. The combined ethereal extracts are dried over sodium sulfate and evaporated in vacuo to leave 2-azido-2-methoxyacetic acid (8.82 g.) as a clear liquid.

後処理

  1. temperatureThe mixture becomes warm and cloudy during the addition
  2. customThe methanol is removed under reduced pressure
  3. extractionextracted with ether
  4. dry with materialThe combined ethereal extracts are dried over sodium sulfate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-44b71b0eef774d209f3f4bd62c86c095
出典データセット
uspto-grants-1976_06
特許番号
US03962224

反応ノート

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